EP2441821A1 - Particules de détergent pour le lavage du linge - Google Patents

Particules de détergent pour le lavage du linge Download PDF

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Publication number
EP2441821A1
EP2441821A1 EP10187518A EP10187518A EP2441821A1 EP 2441821 A1 EP2441821 A1 EP 2441821A1 EP 10187518 A EP10187518 A EP 10187518A EP 10187518 A EP10187518 A EP 10187518A EP 2441821 A1 EP2441821 A1 EP 2441821A1
Authority
EP
European Patent Office
Prior art keywords
detergent particle
coated detergent
surfactant
coated
particle according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP10187518A
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German (de)
English (en)
Inventor
Stephen Thomas Keningley
Jonathan Osler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unilever PLC
Original Assignee
Unilever PLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unilever PLC filed Critical Unilever PLC
Priority to EP10187518A priority Critical patent/EP2441821A1/fr
Publication of EP2441821A1 publication Critical patent/EP2441821A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/046Salts
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/37Mixtures of compounds all of which are anionic
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/10Carbonates ; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50Perfumes
    • C11D3/502Protected perfumes
    • C11D3/505Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay

Definitions

  • the present invention relates to large laundry detergent particles.
  • CA 23000786 discloses that by adding a co surfactant to MES it is possible to lower the Kraft point of the MES and hence provide better dissolution of a MES detergent in a cold water wash medium.
  • WO2009/050026 discloses that by adding a co surfactant to MES it is possible to lower the Kraft point of the MES and hence provide better dissolution of a MES detergent in a cold water wash medium.
  • WO9932599 describes a method of manufacturing laundry detergent particles, being an extrusion method in which a builder and surfactant, the latter comprising as a major component a sulphated or sulphonated anionic surfactant, are fed into an extruder, mechanically worked at a temperature of at least 40°C, preferably at least 60°C, and extruded through an extrusion head having a multiplicity of extrusion apertures.
  • the surfactant is fed to the extruder along with builder in a weight ratio of more than 1 part builder to 2 parts surfactant.
  • the extrudate apparently required further drying.
  • PAS paste was dried and extruded.
  • Such PAS noodles are well known in the prior art. The noodles are typically cylindrical in shape and their length exceeds their diameter, as described in example 2.
  • US 7,022,660 discloses a process for the preparation of a detergent particle having a coating.
  • the present invention provides a coated detergent particle that is a concentrated formulation with more surfactant than inorganic solid. Only by having the coating encasing the surfactant which is soft can one have such a particulate concentrate where the unit dose required for a wash is reduced. Adding solvent to the core would result by converting the particle into a liquid formulation. On the other hand, having a greater amount of inorganic solid would result in a less concentrated formulation; a high inorganic content would take one back to conventional low surfactant concentration granular powder.
  • the coated detergent particle of the present invention sits in the middle of the two conventional (liquid and granular) formats.
  • Alkyl ester fatty acids tend to be crystalline surfactants.
  • co-surfactant such as an anionic and/or non-ionic to alkyl ester fatty acids results in the mixture being an amorphous form rather than crystalline; the amorphous form is sticker than the crystalline form which results is processing negatives and caking on storage.
  • the present invention provides a coated detergent particle having perpendicular dimensions x, y and z, wherein x is from 1 to 2 mm, y is from 2 to 8mm (preferably 3 to 8 mm), and z is from 2 to 8 mm (preferably 3 to 8 mm), wherein the particle comprises:
  • alkyl ester fatty acid as found herein is to the sodium salts thereof.
  • wt % refer to the total percentage in the particle as dry weights.
  • the present invention provides a coated detergent particle that is a concentrated formulation with more surfactant than inorganic solid. Only by having the coating encasing the surfactant which is soft can one have such a particulate concentrate where the unit dose required for a wash is reduced. Adding solvent to the core would result by converting the particle into a liquid formulation. On the other hand, having a greater amount of inorganic solid would result in a less concentrated formulation; a high inorganic content would take one back to conventional low surfactant concentration granular powder.
  • the coated detergent particle of the present invention sits in the middle of the two conventional (liquid and granular) formats.
  • the co-surfactant is other than MES.
  • the coated laundry detergent particle is curved.
  • the coated laundry detergent particle may be shaped as a disc.
  • the coated laundry detergent particle does not have hole; that is to say, the coated laundry detergent particle does not have a conduit passing there though that passes through the core, i.e., the coated detergent particle has a topologic genus of zero.
  • the alkyl benzene sulphonate may be branched for example tetrapropylenebenzenesulphonate or linear for example linear alkyl benzene sulphonate.
  • the alkyl benzene sulphonate is linear alkyl benzene sulphonate.
  • the sulphonated alkyl ester may be pure alkyl ester sulphonate or a blend of a mono-salt of a sulphonated alkyl ester of a fatty acid having from 16 to 26 carbon atoms where the alkyl portion forming the ester is a straight or branched chain alkyl of 1 to 6 carbon atoms and a disalt of a sulphonated fatty acid.
  • the ratio of monosalt to disalt being at least 2:1 and up to about 25:1.
  • the sulphonated alkyl esters used are typically prepared by sulphonating an alkyl ester of a fatty acid with a sulphonating agent such as SO 3 .
  • the sulphonated alkyl esters When prepared in this way the sulphonated alkyl esters normally contain a minor amount of the disalt of the sulphonated fatty acid which results from hydrolysis of the ester. Preferred sulphonated alkyl esters contain less than about 10% by weight of the disalt of the corresponding sulphonated fatty acid.
  • the sulphonated alkyl esters include linear esters of C16 to C26 carboxylic acid which are sulphonated with gaseous SO 3 according to the Journal of American oil Chemists Society 52 (1975) pp 323-329 .
  • Suitable starting materials would include natural fatty substances as derived from tallow, palm oil, coconut etc.
  • MES type methyl ester fatty acid sulphonate
  • the IUPAC name for e.g. a so-called C16 MES is Hexadecanoic acid, 2-sulfo-, 1-methylester, sodium salt (C17H33NaO5S).
  • Methyl ester sulphonate can be obtained by sulphonation of various renewable oleo-based methyl ester feedstocks derived from e.g. coconut (C12-14), palm kernel (C8-18), palm stearin (C16-18) or tallow (C16-18).
  • MES is of special interest due to good biodegradability, detergency and calcium hardness tolerance.
  • ⁇ -Sulfofatty acid esters can be prepared from a variety of sources, including beef tallow, palm kernel oil, palm kernel (olefin) oil, palm kernel (stearin) oil, coconut oil, soybean oil, canola oil, cohune oil, coco butter, palm oil, white grease, cottonseed oil, corn oil, rape seed oil, soybean oil, yellow grease, mixtures thereof or fractions thereof.
  • Suitable fatty acids to make ⁇ -sulfofatty acid esters include, but are not limited to, caprylic (C 8 ), capric ((C 10 ), lauric (C 12 ), myristic (C 14 ), myristoleic (C 14 ), palmitic (C 16 ), palmitoleic (C 16 ), stearic (C 18 ), oleic (C 18 ), linoleic (C 18 ), linolenic (C 18 ), ricinoleic (C 18 ), arachidic (C 20 ), gadolic (C 20 ), behenic (C 22 ), and erucic (C 22 ) fatty acids.
  • ⁇ -Sulfofatty acid esters prepared from one or more of these sources are within the scope of the present invention.
  • Samples of alkyl ester fatty acid sulphonate surfactant prepared in dry powder formed via above mentioned production processes typically contain about 75-85 % by weight of the desired surfactant on surfactant.
  • the water soluble inorganic salts are preferably selected from sodium carbonate, sodium chloride, sodium silicate and sodium sulphate, or mixtures thereof, most preferably 70 to 100 wt % sodium carbonate on water soluble inorganic salt.
  • the water soluble inorganic salt is present as a coating on the particle.
  • the water soluble inorganic salt is preferably present at a level that reduces the stickiness of the laundry detergent particle to a point where the particles are free flowing.
  • the amount of coating should lay in the range 1 to 40 wt % of the particle, preferably 20 to 40 wt %, even more preferably 25 to 35 wt % for the best results in terms of anti-caking properties of the detergent particles.
  • the coating is applied to the surface of the surfactant core, by crystallisation from an aqueous solution of the water soluble inorganic salt.
  • the aqueous solution preferably contains greater than 50g/L, more preferably 200 g/L of the salt.
  • An aqueous spray-on of the coating solution in a fluidised bed has been found to give good results and may also generate a slight rounding of the detergent particles during the fluidisation process. Drying and/or cooling may be needed to finish the process.
  • the thickness of coating obtainable by use of a coating level of say 5 wt% is much greater than would be achieved on typically sized detergent granules (0.5-2mm diameter sphere).
  • this surface area to volume ratio must be greater than 3 mm -1 .
  • the coating thickness is inversely proportional to this coefficient and hence for the coating the ratio "Surface area of coated particle" divided by "Volume of coated particle” should be less than 15 mm -1 .
  • the coated detergent particle has a core to shell ratio of from 4 to 1:1, most preferably 3 to 1.5:1; the optimal ratio of core to shell is 2:1.
  • MES/LAS paste was dried as described previously,(2) to a range of moisture contents and material assessed for milling and dissolution behaviour.
  • the MES/LAS mixtures were dried to moisture contents in the range 1.66% to 2.62%. All of these materials were found to be millable in agreement with the earlier lab-based results. Examination of dissolution behaviour 'as-made' and after storage at 52%RH also found all to be acceptable, with T90 values increasing with MES moisture content. These results seem to confirm the earlier lab-based study however further storage work at elevated temperature,(26°C) such as would be regularly experienced in Asia found a marked tendency for the material to soft cake even in sealed containers. This behaviour means that an 80/20 MES/LAS blend is not acceptable for incorporation in laundry detergent powders.
  • Surfactant raw materials were mixed together to give a 67wt% active paste comprising 80 parts MES and 20 parts LAS.
  • the dried surfactant blend dropped onto a chill roll, where it was cooled to less than 30°C.
  • the cooled dried surfactant blend particles were milled using a hammer mill.
  • the resulting milled material is hygroscopic and so it was stored in sealed containers.
  • the cooled dried milled composition was fed to a twin-screw co-rotating extruder fitted with a shaped orifice plate and cutter blade.
  • the average particle diameter and thickness of samples of the extruded particles were found to be 4.8 mm and 1.2 mm respectively.
  • the standard deviation was acceptably low.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Detergent Compositions (AREA)
EP10187518A 2010-10-14 2010-10-14 Particules de détergent pour le lavage du linge Withdrawn EP2441821A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP10187518A EP2441821A1 (fr) 2010-10-14 2010-10-14 Particules de détergent pour le lavage du linge

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP10187518A EP2441821A1 (fr) 2010-10-14 2010-10-14 Particules de détergent pour le lavage du linge

Publications (1)

Publication Number Publication Date
EP2441821A1 true EP2441821A1 (fr) 2012-04-18

Family

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EP10187518A Withdrawn EP2441821A1 (fr) 2010-10-14 2010-10-14 Particules de détergent pour le lavage du linge

Country Status (1)

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EP (1) EP2441821A1 (fr)

Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2480579A (en) * 1943-10-21 1949-08-30 Colgate Palmolive Peet Co Detergent products and their preparation
US4671900A (en) 1980-12-19 1987-06-09 Henkel Kommanditgesellschaft Auf Aktien Preparation of light-colored, wash active α-sulfofatty acid
US4816188A (en) 1984-10-20 1989-03-28 Lion Corporation Process for the preparation of saturated/unsaturated mixed fatty acid ester sulfonates
US5329030A (en) 1990-11-12 1994-07-12 Henkel Kommanditgesellschaft Auf Aktien Process for the production of concentrated aqueous dispersions of α-sulfofatty acide mono- and/or disalt
US5382677A (en) 1990-05-30 1995-01-17 Henkel Kommanditgesellschaft Auf Aktien Process for the production of highly concentrated pastes of α-sulfofatty acid alkyl ester alkali metal salts
US5384422A (en) 1990-05-30 1995-01-24 Henkel Kommanditgesellschaft Auf Aktien Process for the production of light-colored α-sulfofatty acid alkyl ester alkali metal salt pastes
US5587500A (en) 1993-09-17 1996-12-24 The Chemithon Corporation Sulfonation of fatty acid esters
WO1999032599A1 (fr) 1997-12-19 1999-07-01 Manro Performance Chemicals Limited Procede de production de particules
CA2300078A1 (fr) 1998-06-08 1999-12-16 Gerrard M. Carlson Les variations du rythme cardiaque indicatrices de la capacite d'exercice
US6057280A (en) * 1998-11-19 2000-05-02 Huish Detergents, Inc. Compositions containing α-sulfofatty acid esters and methods of making and using the same
WO2000053719A1 (fr) * 1999-03-09 2000-09-14 The Procter & Gamble Company Particules de detergent enrobees ou partiellement enrobees de couches
EP1081219A2 (fr) * 1999-09-03 2001-03-07 Cognis Deutschland GmbH Détergents sous forme solide
WO2005000026A1 (fr) 2003-06-30 2005-01-06 Valrom Industrie S.R.L. Recipients en materiaux thermoplastiques a proprietes bactericides
US7022660B1 (en) 1999-03-09 2006-04-04 The Procter & Gamble Company Process for preparing detergent particles having coating or partial coating layers
WO2009050026A2 (fr) * 2007-10-17 2009-04-23 Unilever Nv Compositions de blanchisserie

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2480579A (en) * 1943-10-21 1949-08-30 Colgate Palmolive Peet Co Detergent products and their preparation
US4671900A (en) 1980-12-19 1987-06-09 Henkel Kommanditgesellschaft Auf Aktien Preparation of light-colored, wash active α-sulfofatty acid
US4816188A (en) 1984-10-20 1989-03-28 Lion Corporation Process for the preparation of saturated/unsaturated mixed fatty acid ester sulfonates
US5382677A (en) 1990-05-30 1995-01-17 Henkel Kommanditgesellschaft Auf Aktien Process for the production of highly concentrated pastes of α-sulfofatty acid alkyl ester alkali metal salts
US5384422A (en) 1990-05-30 1995-01-24 Henkel Kommanditgesellschaft Auf Aktien Process for the production of light-colored α-sulfofatty acid alkyl ester alkali metal salt pastes
US5329030A (en) 1990-11-12 1994-07-12 Henkel Kommanditgesellschaft Auf Aktien Process for the production of concentrated aqueous dispersions of α-sulfofatty acide mono- and/or disalt
US5587500A (en) 1993-09-17 1996-12-24 The Chemithon Corporation Sulfonation of fatty acid esters
WO1999032599A1 (fr) 1997-12-19 1999-07-01 Manro Performance Chemicals Limited Procede de production de particules
CA2300078A1 (fr) 1998-06-08 1999-12-16 Gerrard M. Carlson Les variations du rythme cardiaque indicatrices de la capacite d'exercice
US6057280A (en) * 1998-11-19 2000-05-02 Huish Detergents, Inc. Compositions containing α-sulfofatty acid esters and methods of making and using the same
WO2000053719A1 (fr) * 1999-03-09 2000-09-14 The Procter & Gamble Company Particules de detergent enrobees ou partiellement enrobees de couches
US7022660B1 (en) 1999-03-09 2006-04-04 The Procter & Gamble Company Process for preparing detergent particles having coating or partial coating layers
EP1081219A2 (fr) * 1999-09-03 2001-03-07 Cognis Deutschland GmbH Détergents sous forme solide
WO2005000026A1 (fr) 2003-06-30 2005-01-06 Valrom Industrie S.R.L. Recipients en materiaux thermoplastiques a proprietes bactericides
WO2009050026A2 (fr) * 2007-10-17 2009-04-23 Unilever Nv Compositions de blanchisserie

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JOURNAL OF AMERICAN OIL CHEMISTS SOCIETY, vol. 52, 1975, pages 323 - 329
THE JOURNAL OF AMERICAN OIL CHEMISTS SOCIETY, vol. 52, 1975, pages 323 - 29

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